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Diisopropylethylamine → 2-(4-Ethoxy-3-methoxy-phenyl)-N-{2-[2-methyl-6-(2,4,6-trimethyl-phenylamino)-pyrimidin-4-ylamino]ethyl}-acetamide

HRID 2121617
ノート
印刷プレビュー

反応式

HRID 2121617 の反応式
[NH2:1][CH2:2][CH2:3][NH:4][C:5]1[CH:10]=[C:9]([NH:11][C:12]2[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=2[CH3:20])[N:8]=[C:7]([CH3:21])[N:6]=1.[CH2:22]([O:24][C:25]1[CH:33]=[CH:32][C:28]([CH2:29][CH2:30]N)=[CH:27][C:26]=1[O:34][CH3:35])[CH3:23].C(N(CC)C(C)C)(C)C.F[P-](F)(F)(F)(F)F.N1([O:61][P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>C(Cl)Cl>[CH2:22]([O:24][C:25]1[CH:33]=[CH:32][C:28]([CH2:29][C:30]([NH:1][CH2:2][CH2:3][NH:4][C:5]2[CH:10]=[C:9]([NH:11][C:12]3[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=3[CH3:20])[N:8]=[C:7]([CH3:21])[N:6]=2)=[O:61])=[CH:27][C:26]=1[O:34][CH3:35])[CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 1420764-Ethoxy-3-methoxyphenethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 22034099(2-Aminoethyl){2-methyl-6-[(2,4,6-trimethylphenyl)amino]pyrimidin-4-yl}amine

生成物 1

HCID 220341212-(4-Ethoxy-3-methoxy-phenyl)-N-{2-[2-methyl-6-(2,4,6-trimethyl-phenylamino)-pyrimidin-4-ylamino]ethyl}-acetamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of (2-aminoethyl){2-methyl-6-[(2,4,6-trimethylphenyl)amino]pyrimidin-4-yl}amine (0.36 g, 1.26 mmol), 4-ethoxy-3-methoxyphenethylamine (0.26 g, 1.26 mmol)) and N,N diisopropylethyl amine (0.24 ml, 1.38 mmol in CH2Cl2 (5 mL), add benzotriazol-1-yloxytris-(dimethylamino)phosphonium hexafluorophosphate (0.61 g, 1.38 mmol) and stir at ambient temperature for 14 h. Dilute the resulting mixture with CH2Cl2 (20 mL), and wash with water (20 mL) and saturated aq NaCl (20 mL). Dry the organic layer over Na2SO4, filter and concentrate in vacuo. Purify by preparative TLC (7% methanol-CH2Cl2) to obtain the title compound.

後処理

  1. washwash with water (20 mL) and saturated aq NaCl (20 mL)
  2. dry with materialDry the organic layer over Na2SO4
  3. filtrationfilter
  4. concentrationconcentrate in vacuo
  5. customPurify by preparative TLC (7% methanol-CH2Cl2)

出典と根拠

ORDレコード
ord-21cf54611d994cfa8eea4baaafbc8e4f
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06696445B2

反応ノート

読み込み中…

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